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ORNL-
366
9
FREPflEWTION OF k CESIUM
( 3 7 C ~ )
BOROSILICATE GLlSS
POWER SOURCE
C .
L. O t t i n g e r ,
E.
E . P i e r c e , and R. W.
Schaich
Isotopes Division
APRIL 1965
OAK
RIDGE
NATIONAL
JABOLUTORY
Oak
Ridge,
Tennessee
operated by
UNION
CARBIDE
CORPORATION
f o r the
U. S. ATOMIC EW3GY CONMISSION
3 4 4 5 b 0548240
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Page
. . . . . . . . . . . . . . . . . . . . . . . . . .
1
os tmct
. . . . . . . . . . . . . . . . . . . . . . . . 1
ntroduct ion
2
hemical
Processing . . . . . . . . . . . . . . . . . . . .
Source Fabrication
P e l l e t i z a t i o n
. . . . . . . . . . . . . . . . . . . . . 4
. . . . . . . . . . . . . . . . . . . . .
4
Encapsulation
. . . . . . . . . . . . . . . . . . . . .
5
Assembly and Measurements
. . . . . . . . . . . . . . .
5
References . . . . . . . . . . . . . . . . . . . . . . . . . 13
Appendix.. . . . . . . . . . . . . . . . . . . . . . . . . 14
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C . 5;. Ot t inger
E .
14
Pierce
R ,
bJ.
Schaich
37
A
cesium
(
CS) ‘boros i l i ca te sass powr source wii;’t.i 125
watt:;
tl-ierrrml
output was prepared
a t
-the
Isotopes
Development Center, O a k Ricl.ge National h b o r a t o r y
( O R N I L )
.
Techniques
for
the
p r e p r a t i o n of
‘the
u e l matei-Tal.,
i t s
casking
i n t o t h e p ro pe r
foi-11,
and the
fabrication
of
-the
f inal source capsules were developed,
This
paper descr ibes
t he chemical. proc essin g, fuel. pre pa rat ion , source
enxapsu-
l a t i o n ,
heal;
output measurements,
capsule l e ak - r a t e
d e t e r -
minutions, and measurervents on
t h e l o a d e d
skipping cask.
INTRODUCTION
I n 1961
a
program was initiated a t t h e ORNL Isotopes Development Center
t o
develop
techniques for the preparakion
of
a 1-25-mtt
( t h c m a l )
137Cs power
source fo r use i n an
m6 e r w a
C I ~ J ~ J ~ ~ ~ E I ~ ~ ~ O T ~he prP fe r red f u e l Por~ri
would
contain
ti?? 137Cs
i n
a glass v i t h
the h ighes t p rac t ica l power dens i ty
arid
a l o w l e ach
r a t e
i n
sea.
water.
Fused cesium ( l S 7 C s ) a luminos i l i ca te w a s cons iaered as a S O U T C ~mate r i a l
s ince 2 ha6 been shown t o have low s o l u b i l i t y i n most
aqueous
systcms and
t o
have a n eg l i g i b l e r e l e a s e of
137Cs
a t elevated temperntures . l
However,
t he 137Cs
concen t rat ion i n
cesium (137Cs)
aluminos i l icatc i s t o o low
(6-‘(
cur ies /g )
f o r
ap p l i c a ti o n s r eq u i r i n g
a
concentrated
he t
source;
s o
t h e
inves t iga t ion of 137~s source materials was extended t o the cesium
g ~ u s s e s
Culcir iation of cesium tetrapheny lboron i n
a i r
y i e l d s
C S ; ~ Q . B & ~ ~
be reacted with Si02 a t high temperature t o produce ces ium boros i l icate
glass .
A l l of
t h e
operations can be carried out by remote manipulator c e l l
operations.
borosilicate glass
was se lec ted
which
can
For t h i s r e as on
cesium
137Cs
.
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2
as tlie
fml .
fomi
for
t h i s p r o j ec t , and t h e deve1,opmcnt
O S
a manufacturing
process
for t h i s m a t e r i a l
w a s
undertaken.
CHEMIC
AI,
PR
W E
NG
Prior
t o fu3.1-scale processing a t the Fission Products Development
Laboratory,
a
s e r i e s
of
experimental. crsi1.m gl.ass
preparations
was m. ie.
These included the preparat ion of i n ac t i v e
cesium
g lasses 'Graced
w l - t h
137Cs,
w i t h cesium contents ranging from 30-55 h ,;, and t h e p r ep am t i o n
o f
sma3 . l
amounts
of
i ~ ~ l yc-Live cesium (137~s)
orosilicate g3.a.::~
i n a
hot
cell.
On t'ne
bas is
of
t h e
resul.ts
o f these
experimental
runs, a
flow sheet (Fig. 1.) w a s developed Lo produce cesium
(
13'Cs) borosilica-t;z
g lass
v i t l i
a
cesium
content o f h.5-50wt ,;$.
one - t h i r d
of
khe atoms i.n fission-psodirc-f; cesium a r e 137Cs.
w a s as
rfoll.ows.
I t
w i l . l
be
r eca l led tha t abou t
The procedure
1.
Product-grad.e
fission-product . 3 7 C ~ @ l ( 3 3 cu r i e s
of
13"%sper
gram of c e s i m )
was
dissolved i n 0,L
M
a c e t i c
a,cLd
e
3 .
The
s l - u r y
vas
heated t o -(O C and sodium te t raphcnyl-
boron,
at
a
r a t l o
of
3.2 gi-iuns ~ i e r ;iTrm o f
cesium, vas
added.
4.
'Che system was cooled to 30°C; t h en t h e s l u r r y was
fil
ered
through
a
medium po ros ity - al.widim Ti l t c r
t'iiimblz
.
Nine preci.pi-tations we:^'^ necessary
I.n
ord.er
t o
yield.
s u f f i c i e i i t material t o
complete th e sourc e. The major opera t iona l problem thai; w a s encountered
dinring -the first
few
ruiis
was the tendency
of the
cesium tetraphenylboron
p r e c i p i t a t e
t o
s t i c k
t o
.Line
w d . 1 ~
f
the p r e c i p i t a t o r . Since
the
p r e c i p i t a t e
c o u l ~ I
ot be washed
o f f
t h e p r e c i p i t a t o r
m b l s
by normal water
spray flushing,
the
qiumtiitier, o f chemicals added had.
to
be
var ied
from
b a t c h
t o hatch
i n o%(ier
o mainta in
the desired
l3''Cs content
i n
t h e f i n a l
glass. Adjustment;
of the
ag i ta t i on and
tmshing
cycles r e s u l t zd
I.n an
operating procedure which T.WS used suc ces sful ly on the l a s t
four runs,
The
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3
O R N L - D W G
64-7054
**
SE 0 2
0.1
N
ACETIC ACID
3-7 *
SODIUM TET RAP HEN YL BORON CsCl
PR EC PITAT ION
- 2.5
g / l i t e r CE S I UM
-v 8
g / l i t e r
SODIUM
T E T R A P H E N Y L BORON
*
BATCH SIZES: 2000 curies
TO
5 4 0 0 c u r i e s OF
137Cs
SiO, ADDITION S VARIED
TO PRODUCE AVERAGE
ACTIVITY CONCENTRATION
O F -15.5 curies/q IN FINAL
PRODUCT
**
FILTRATE
TO
WASTE TREATMENT
HOT-OFF-GAS TO
W A S TE TRE A TM E NT
HOT- OFF-GAS TO
W A S TE TRE A TM E NT
A S S A Y A ND
M E A S U R E M E N T S
Fig. 1. Cesiwti-137 Borosilicate Glass ProJec t - Flow Diagram
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4
y i e l d
w a s
$$,
as
shown i n
Table
1,
w i t h
most of the
l o s s
i n equipment,
holdup
Table
1.
C e s i u m ( TCs)
boros il . i ca te p rcc ip i ta thxxs
-__-
.......
lll llalcine l...pre......c i p i t a t c
. ___....-
A ct i v i t y
Hatch S t a r t i n g 13'cs
Weight coincent
rat
i011 Total.
number ana lys i s , cur ies cur ies /g cur i es
1
2
5
6
9
Tota.ls
4
940
2,760
2,050
4,200
-I. ,500
2
000
4 '(00
5,200
35,750
_;,400
315.0
1.65
0
131
0
26 5
285
2
126
8
276
0
305 0
322,
2>2.92
13.5
15.0
15.0
15.0
15.0
1'7.0
17.0
17.0
l (.
4,250
1,960
2
-C'(O
I t ,
2 7980
2 ~ 6 0
4,630
3 h ,
3ho
S x
cesiun
sel ec te d batches of t he calci ned powder i n a Waring
Blend.or.
The C O I ~ ~ T J O S ~ ~ ~ S
w r e
loaded
i n t o
platinum cups;
-then th ey were
melted
individ .ual ly in s m a . l l
furnaces
a t l 2 O O 0 C f o r 3
hr.
l3'@s)
boros i l icate composi tes
were
prepared by blending
The s i x
melts weye weighed and
measurerl, and
t h e excess
platinum
was
removed by trimming with
a
shmp ki.if'e,
and mechanical los ses (ca lcu lat ed from veight-I.oss measurements) w a s
approxjimately 2,5013
cilri.es
(-10 ).
Ilea% out;put
ii1easvremenl;s were r i m
on
t h e Tndj.vid.ual rnclts
using
caLnrdrnet r ic tech niqu es developed by Posey e t
al_.s Yfle
d . a t a p e r t a h i n g t o Ynese
glass
r n e l k s are listed
i n
Table
2.
Since
the dens i ty va lues
are
based
on. m%.r;..imwa
dimensions, they are lower
than the t iwe physical.. ensity
of
t he gIass,
from
0.1.9
watts/m3,
t o
0.24
w a t t s / m L ,
i s
probably representa. t ive
for
a
series
o f cesi1m ( l S 7 C s ) horos il . i ca te g las ses
made
by -Lhz
technique
described.
The
'tokal 3?Cs
l o s s by v o l a b i l i t y
The
range of
power density,
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Table 2.
Data on cesium ( l S 7 C s ) b o r o s i l i c a t e glass melts
Activi ty Heat Power
tk ig ht , Dens i ty , concentra t ion, cmtput den s i t y ,
Tota l
nutiber g l d cw i e
s / g
watts 137~s
w a t t s l a
c u r i e s
l 232.0
3.06
13.
I 14.41
0.19 3,200
2 316.0
3.24 14.8
20.58
0 . a 4,670
3 316.4
3.16
14.8
20.61
0.21
4,690
4
308.5
3.05
16.1
24.45
0.24 4,970
281.2
3.02 16.1
22*3 ,
0.24 4,550
b 2E . B
3.00
16.1 22.613
0.24
4,600
1
(40.9 125.10 26,680
Encapsulat ion
The s i x completed
cesium
(13-'Cs) b o r o s i l i c a t e glass melts (Fig. 2 ) were
loaded
i n t o two I l as te lloy inn er
capsl-iles.
The inner
capsules were
velded
rerfiotely
(p ig . 5)
under argon containing "KT t r a c e r .
~ a c ~ i
nner capstfie
was cleaned and Leak- tes ted f o r 85Ki,.
The inner capsules were inserbed
into
Xlsstelloy
oiiter
caps ules which were then welded remotely
under
wgon
with
KY
tr a ce r, The completed caps ules (Fig. 4) e r e l e a k - t e s t e d f o r
Kr,
then
cleaned. o an average smear count
of'<200
d/min f o r
a
sing1.e
smear over t h e en t i r e s u r f ace .
All of
t h e
l e a k
ra tes ,
determined
by thc
fi
tracer
niettioci.,
~iez le
elow
the
limit
of
detection
of
oW@t
n i ~ l y e a r
s ee
il-ppendizr
.
85
Assembly
and
Measmementc
@a3,1.0r.ime"Lic
mneasusements
on t h e cornpleted capsules showed 55.6 watts for
No.
1
and. 69,5 wa t t s
f o r No.
2.
Capsule
;No. 1 ms placed i n the bot tom of
t h c c a v i t y of
a
l?.O-in.-thick depleted
uranium
s h i e l d (Fig.
5 ) ,
and capsule
No.
2 w a s placed on t o p of capsule No. 1. The fr e e space above tile capsules
was approximately 1/8 in .
Thrce thermocouples were a t t a ch ed
t o
the shield--one on the bottom and
t w o
on oppos ik sides
of the
c y l i n d r i c a l p o r ti o n . A s shown i n Table 3, t h e
shrielcl
surface
temperature
was
f a i r l y uniform, w i t h
the
ternperatwe on t h e
boikom
surface running s l i g h t l y
l e s s
t h a n t h a t on t h e s i d e s .
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I
,
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9
Fig.
5.
Fuel Loading
of
Cesium (137Cs) Borosilicate Power Source
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1
Table 3 .
Cesium (
137Cs
) borosi l icate power 'source
temperature measurements
May 28,
1962
my 29, 1@2*
oc
**
Time, Temp, Time, Temp,
c **
min Bottom Side Side
min
Bottom Sid e Sid e
0 80
88 83
72 80 80
1 5 81 85 85
15 io- 81
81
30 83
85
85
30 n
81 83
45
83
86 85
45 80 82
83
60 83
86
86
60
80 82 4.
*
**
These readings were taken with the shield resting on wooden blocks.
Ambient temperature w a s 30°C i n a l l cases.
The
uranium
s h i e l d w a s placed i n th e shipping cask (Fig. 6) nd allowed t o
remain overnight t o measure th e temperature under t ran sp ort condit ions.
Table 4 ives the temperatures thus measured; they showed that no tempera-
t ur e problems should be expected during tr an sp or t.
Table 4.
Cesium
(137Cs)
bo ro si l i ca te power source
shipping cask temperatures
L
Temp,
C
Time, Between ca sk Cask
hr Ambient and sh ie ld surfac e
____. _
I
0
1 7 - 5
16.25
18.25
30
27
27
28
72
72
72
71
30
41
41
41
The uranium shield
w a s
removed from the shipping cask and placed on
i t s
s id e
i n two wooden
V
blocks.
s h i e l d i n his a t t i t u d e .
The
r e s u l t s of these measurements and the
ca lcu la ted va lues
are
shown i n Table
5.
The agreement between the calcu-
lated and observed readings
w a s
s a t i s f a c t o r y
for
a
source
of
t h i s
s i z e
and
shape.
Radiation measurements were taken with the
-k
Smears
for
surface contamination were made on the uranium shield, the
inside of the shipping cask, and the
sur face
of
the shipping cask
just
p r i o r
t o lo adin g f o r shipment. In a l l cases the con taminat ion leve l was <20 d/min
alpha and <500 d/min beta-gamma.
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i
11
PH O TO 577 7
Fig. 6 . Uranium
o s i l i c a t e Power Sou
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12
Table 5.
Cesium (137Cs) bo ro si l i ca te power source
radiation measurements
Distance from
s h ie ld , em
Rad ia t ion ( s ide ) ,
mr/hr
Calculated Observed
Radiation (e nd ), mr/hr
Calculated Observed
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1.
R. E .
Lewis, Reported i n
ORNL
progress repor ts and
s m n r i z e d i n
"Glasses"
Isotopes
and Radiation Technology,
1:81+
(Fa l l
1963).
2.
T,
C .
Quinby, Method
of
preparing radioact ive cesium
SQUTC~S,
U,
S.
Patent 3,114,716,
Dee. 17,
1963.
3 . J , C. Posey, T. A,
But le r ,
and P. S.
Baker, Hot c e l l calor im etry
f o r rout ine determination of thermal power genera ted by ki loc uri e
sources, Proceedings
_I_.
f the Tenth Conference on H o t $ahorator ies
and_ Equipment, Washington, D, C .
Nuclear Society.
1962 , pp. 2b5-m merican
4.
E. D. Arnold m d
B.
F. &skewitz, SDC - A sh ie ld in g des ign ca l cu -
la t ion code f o r f u e l h an dl in g f a c i l i t i e s
(A
smrking but incomplete
program
fo r
Vne
IBM-7090,
t o be publ i shed
as
ORNL-3041).
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All
o f
Liir
s o u c c
capsules K J C ~ elded in a sealed weldel*
ixndcr
argon.
'Yh
following
procediux
was
used,
1.
2.
3 .
-L .
5.
6 .
> .
8 .
9.
The capsule, w i t h
a
p r p s s - f i t cap, w a s i n s e rt e d i n t o t h e
wclder, and the welder was sealed. The
capsule
cap was
scored t o permit transfer o f atmosphere betwpm the welder
&nil thc. capsule.
Tnc:
welder ~~8.smr:mtGed
nd
r e f i l l e d s i x t imes
hrii Ii
dry
argon. 'Then
3.1,
w a s pressur ized
t o
three atmospheres w%th
argon containing two
cimizs
of 8
The
cnpsifl-e w a s
welded.
The
capsule
was i-eninvccl f r 9 m
-the welder, aid t h e
wzld ~ i a s
i cispec
Led
visin_lly,
'The surface o f
Lhe capsule
was
cleaned.
The capsule w a s i n s e r t e d i n t o
.the
l e ak de t e c t o r
(a
sca led
cliamber having vaJ..vsd l i n e s to mcuim
ind argon supply and
cozmcctcd tiirou@ a valve .to 8,s). evacuated cow-Ling chmd,cr).
The
l e a k
de tec to r
was
evacuated
and
refilled
w i t h
d i ~ y rgon
foiir
tinies.
pres
su re .
Then I.-
as : f i l l e d
with argon
xL ztmospheric
The'
capsule
msallowed
t o
r c m i n i n
t h e l e a k
dc tcc to r for
fo u r
hours .
pass through any
leaks
i n the capsule and mix with t h e argon
i n the leak detector .
T;x mixed A r - 8sK r i n tile capsule cowl-d thus
The valve betveen M E 3.eizk de tec to r and the evacuated
cou i t ing cimbelg
t m b
opencil, and t h e system
was
al . lowd to
stabilize.
The counting chamber vas the a seaJ-ed, removed
from
the
system, &nil the
~ r s
counted,
The
fol lowing
csl.culations were ma& t o
d e t e m i n e I.eak
r a t e
:
Free volunz of
welder
12.2
l i t e r s
Free volume of
l e a k
dekector
1.08 l i k r s
VoJ-me of counting chamber
1.07
l i t e r s
Presswe o f welding gas ;i atm
8 5 ~ontent 2QOO rii
Efficiency of counter
( A r
+ R 5 ~ r
l ,
background count =
1(300
-
50 c/Klin
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I
15
a)
Volume of'
welding gas
a t Z a t m
= 36,600
m l
b)
Concentrat ion
of
8*Kr i n
welding 88s
=
c )
D i s i n t eg r a t i o n rate
=
0.055 mc/m;l. x 2.22 x 110'
d / m i n * m c =
12*2
lo7 d/nin*ml.
d)
e )
count
r a t e a t l e f f i c i e n c y =
1 2 . 1 10
/ m i n * d
Tinerefore,
1
c/mrin
= 0.83 x 10 ' mL
f )
Since only 50$ of the l e ak d e t ec t o r g a s 1s
smiplcd,
1
c/min
= 1.66 x
niL
of welding gas
Since
the
back4,rounrl count c m v ar y by
120
c/niin
from nigh o l o w , any count ra te
of
1 20 c / i i ~ n
(equ iva len t t o 2.0 x io-* m~
of
gas)
represenbs
an uncer ta in leak.
count r a t e i s equ iva len t t o
a l e a k
r a t e
of
0.44
ml/year
under
the
cond.it ions described. Tine Limit of
detection may
be 1-educed
by increas ing the accmiu-
l a t i o n
time.
g )
For
a
4-hr accumula t ion , th i s
w h i c h
i s
t h e lowes t l eak rate de-tectable
i
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t
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Library
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5. Reactor Di.vision
Library-
6-7.
ORTn.
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Technical. Library
Document
R e ferenc S e c tLori
8-27.
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Records
Department
28. 1,Bboratory liecords,
QRTU..I
R.C.
29. P. S .
Balier
30. E . E.
Beaueh-amp
3 1 _ .
71. A.
B u t l e r
3 2 .
J.
11. Gi l . l e t t c
33.
K.
W.
Iiaff
34. E .
E. Ke'cchen
EXTEfUAL
DZSTRIBWION
35
H.
IT. L af f e r t y
36. H.
G. MacPherson
37.
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38.
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E.
Larson
39. R.
G.
Niemeycr
40-43. C. L. Ot t inger
4.4. .
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Pie r ce
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Xupp
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48-51. R, Id.
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Weinberg
54-Research.
and
Developen-i;
Division,
AEC,
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55-512.
Given distribution as shown i n TID-45OO (39th ed.) .under
Isotopes -inkus trial
Teelinology category
(75
copies -
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